Eduaed ullrich



UNITED STATES ATENT OFFICE.

EDUARD ULLRICH, OF HCOHST-ON-THEMAIN, ASSIGNOR TO CARL ROTH, OF BERLIN, AND THE FARBWVERKE, VORMALS MEISTER, LUOIUS & BRIINING, OF HOCHST-ON-TIIE-MAIN, GERMANY.

PRODUCTION OF DIMETHYLDIETHYLTHlONlN BLUE.

SPECIFICATION forming part of Letters Patent No. 366,639, dated July 12, 1887,

Application filed January 13, 1887. Serial No. 221,282. (No specimens.) Patented in France December 24, 1885, No. 173,137; in Germany December 25, 1885, No. 38,513, and in England January 1, 1986, N0. 43.

To all whom it. may concern:

Be it known that I, EDUARD ULLnIon, doctor of philosophy, a citizen of the Empire of Germany, residing at IIL chst-onthe-Main, in

the Empire of Germany, have invented certain new and useful Improvements in Dimethyldi ethylthionin-Blue; and I do hereby declare the following to be a full, clear, and exact descrip tion of theinvention, such as will enable others skilled in the art to which it appertains to make and use the same.

This invention relates to a blue dye-stuff or coloring-matter, which I term dimcthyldiethylthionin-blue, the hydrochlorate of dibeing an essential constituent of the same. This blue dye-stuff or coloringmatter I produce byjoint oxidation of paramidodimethyl aniline 0 H, Egggi and 5 in presence of a hyposulphite, precipitating the coloring-matter from its solution by means of zinc chloride or common salt. According to the said process twelve parts of dimethylaniline are dissolved in diluted hydrochloric 3O acid (forty parts of water and sixty-five parts of concentrated hydrochloric acid) and by the addition of seven and one-tenth parts of nitrite ofsodium and subsequent addition ofzinc convcrted into amido-dimethylaniline. Aquan- 3 tity of zinc is added necessary to use up all the free hydrochloric acid. The solution thus obtained is diluted with water to about five hundred parts, and then I add eighteen parts of hydrochlorate of diethylaniline and twentyfiveparts of hyposulphite of sodium. Now,

diethylanil inc I oxidize by adding a solution of twenty-five parts of potassiunrdichromate, boil for about two hours, add the quantity of sulphuric acid necessary to bind the chromoxide and the alkalics, and expel the sulphurous acid by further 5 boiling. Then the dissolved leuco compound is convcrled into the coloring-matter by adding an oxidizing agent, and, finally, it is precipitat ed by means of common salt.

The coloring-matter is a bronze-like powder and of brown color. The blue solution of the same can be easily reduced into a colorless liquid. Oxidizing agents restore the original shade. By means of tannin and emetic tartar the coloring-matter is fixed in the fiber so that it will resist washing. Quicksilver, chloride, and potassiumbichromate precipitate the solution, the precipitate being of a dark-blue color.

The identical eoloringmattcr will be ob- 6o tained by joint oxidation of paramido diethylaniline and dimethylaniline in presence of a hyposulphite. The process for producing the coloringmatter according to this method is analogous to the process described hereinbe' fore.

That I claim as new, and wish to secure by Letters Patent, is-

As a new product, dimethyldielhylthioniir blue produced byjoiut oxidation of parami- 7o do-dimcthylaniline and diethylaniline in presence of'a hyposulphite or of paramido-diethylaniliue and dimethylaniline in presence of hyposulphite, and having the characteristics above set forth.

In testimony whereof I alfiX my signature in presence of two witnesses.

EDUARD ULLRIG H.

Witnesses:

J EAN GRUND, JACOB MUELLER. 

